High temperature high pressure apparatus



JuneZl, 1960 HIGH TEMPERATURE HIGH PRESSURE APPARATUS Filed Feb. 14, 1955 Fig] FQ. Z.

Howard Tracy Ha/,

by /QZ 4. His Attorn ey.

H. T. HALL 2,941,242

HIGH TEMPERATURE HIGH PRESSURE APPARATUS Howard Tracy Hall, Niskayuna, N.Y., assignor to General Electric Company, a corporation 'of New York Filed Feb. 14,19s5,ser.N 0. 488,041 6 claims. (ci. lts-16.5)

My invention relates to high temperature high pressure -stentapparatusand specifically to such apparatus in. which av i gasketlassembly is provided tov increasethe volume of the reaction chamber and thepressure applied thereto.

In a copending applicationl of Francis. P. Bundy; Serial No. 448,042, tiled concurrently herewith and assigned to thezsame assignee as the present application, an .ap-

paratus is described toeiect and control reactions occuring 'at temperatures ofthe order of several vthousand degrees centigrade and pressures of the order of 40,000'to` 60,000' atmospheres for longtime-intervals. -Such apparatus comprises 'a reaction vessel which is positioned between a pair oli-opposed, recessed dies to provide ia specimen chamber to be subjected to temperatures and pressures of the order mentioned.

A high temperature high pressure apparatus which provides a-reaction vessel of increased size is-"desirabl'e to accommodate larger amounts of materialsto be heated and pressed.4 lIn previous devices, the sizeof the reac-A tion vessel was limited by thickness of the insulating and pressure resisting gasket. Such a gasket couldv be increased'in size but application of high pressure caused lateral 'extrusion thereof from between opposed members with attendant loss of f pressure in the reaction vessel. The invention of the present application eliminates such gasket extrusion with a novel gasket assembly which permits an increase in both reaction vesselsize and applied pressure. i

Agicordirigly,` it is an object of the invention to provide a new' and improved hightemperature high pressure` Itis another object of the 'invention tov provide an improved high temperature high pressure' apparatus in which .both the size of .the reaction vessel and applied pressure are increased.

It is a further object of the invention to provide an A ahigh temperature range. Y y,

In carrying out my invention in one for-m, al gasket assembly is positioned around a 4easing within a pair of opposed, recessed -dies to provide an enlarged reaction vessel which is subjected toy high 'temperature and high pressure'.

The'se and various other projects, features and advantages of the invention will 4be bettervunderstoodfrom the Vfollowing `description taken `in; connection with the accompanying drawin-ginwhich: a

improved high 'pressure apparatus which is subjected to Fig. 1 is a front elevational view of a hydraulic press with a high temperature high pressure apparatus which `embodies my invention; and

Fig. 2 is an 'enlarged sectional view of the high tem.

perature high pressure apparatus which is shown in Fig. 1.

In Fig l of the drawing, a hydraulic'press comprises a base 10 with a press bed 11 onwhich is mounted a plurality of vertical shafts 12 to support a carriage A13 with a hydraulic shaft 14. A pair of opposed pistons ice 2- 15 and 16 on bed 11 and carirage v13 are recessed to partially position members 17 therein, each of which members -17 comprises a central die 118 with surrounding binding rings 19. A layer of electrical insulation 20 is provided between at least one member 17 and its associated piston 15 to prevent conduction of electric current through the press. An electrical connection to each member 17 is provided by a conducting ring 21 with a connector 22 which ring is positioned around the periphery o f each outer binding ring 19 to supply electric current from a source of power (not shown) through rings 19 and `dies 18 to the high temperature high pressure reaction vessel which isdescribed below.

As is best shown in Fig. 2, the outer face of each die 18 has a raised annular lip-23 which deines a recess. The lip and recess thus formed are spaced from the periphery of the -face of the die. A block 24 of electri- "cally insulating material is positioned in the central por'- tion of each recess to prevent burning out dies 18 through the application of current thereto. A reaction Vessel 25,

which is located within the recesses of opposing dies 18, comprises a pair of spaced conductive discs 26 with a 'hollow conductive cylinder 27 therebetween adapted to contain a specimen 28 to be'subjected to high temperature high pressure conditions. An annular washer l29 of electrically insulating material is positioned around cylinder 27 between `discs .26 to complete the assembly of reaction vessel 25. If it is desired, reaction vessel 25 may be in the form of a hollow casing which is in electrical contact with opposing dies 18.

An annular gasket assembly 30 surrounds vessel 2.5

tion vessel 25 to which greater pressuresmay be appliedwithout lateral extrusion of gasket assembly 30 with attendant loss of pressure. Such higher pressures are attained with gasket assembly 30 because the non-extruding material increases the length of travel 'of die 18 along its center line todevelop increased pressures. Examples of suitable n iaterials ffrom which blocks 24, and washersv4 I 29 and 31 may beY made are pyrophyllite and catlinite.

'In the operationof the high temperature high pressure lapparatus shown in Figs. l and 2, each member 17 withassociated conducting ring 21 and connector 22 is positioned partially within the recess of its respective pisf ton in thepress. Block 24 is then set in the central portion of the recess of each -die 18 to provide electrical insulation. Specimen -28 which is to be subjected to a high temperature .high pressure environment is placed in cylinder 27 within washer 29 between discs 26 to complete reaction vessel 25. n Gasket assembly v30 is positioned around vessel 25 after which this vessel and its associated -gasket assembly 30 are positioned within the recesses of opposing dies 18 between blocks 24.- The outer edge' of'gasket assembly 30 tits between and is enga-ged by opposed lips 23 to prevent lateral extrusionof this assembly with 'attendant loss of pressure to vessel 25 when' pressure is appliedby the press.

Pressure is applied to substance 28 in cylinder 27 byshaftl 14 of the press. At the same time, electric current is supplied from one electrical connector, such as upper connector. 22'to upper conducting ring 21, binding rings 19, die 18 and upperA disc 26 to generate heat in cylinder 27 of vessel 25. AThe current path continues from cylinder 27 through lower disc 2 6, die 18, lbinding rings 19,A

conducting ring 21, and connector 22 to the electricalV source. Pressures in eucessgof 50,000 atmospheres at temperatures higherf than 25,0()` C. havebeenlmaintainedin-suchapparatus for` periods oivhours, I'fgitisI desired, reaction vessel` 25A may,Y alsobestrbjected to, high pressures-y alone.

As will` be apparent tothoseA skilled in the art, the objectsofimy., invention are attained-bythe use of` a1 .gasketv assembly which is positionedbetweena pair ofv opposed,

What I. claimas new anddesire -tosecureby Letters Patent ofthe United,l States is:

l. High temperature'highl pressure apparatusf comprising.l a-pair of opposed, recessedA` pistons, meansg for' exsv erting pressure against at. least.,V one of said pistons, al

pair of members, one' of said membersbeinggpositioned partially: within each` of -said rece sses,`a1 layer of; insular-- tion between oneof i saidv members, and its associated pis,

ton, an` electrical connection to eachf-offsaidinem-bers,

each member, comprisingal die; thetouter. facefofV said'v die having-a raised annular lip deflninga recess,Y afcylindri cal reaction vessel located within; the -recesses of j opposingdief-faces, said reaction vessel Ibeing'inelectrical confv taotwithtsaid. dies, andan annular gasket assembly s urrounding-` theiside of said' vessel,: said, gasket assembly comprising a pair of annularV insulating-andpressure `resistingi washers, an annular. metallicv washer positioned between said pair-V of.. insulating and pressurei resisting washers, saidv gasket assembly having itsouter edge-positioned adjacent said annular lip,- thef outeredge ofsaid `gasket assembly being arranged -tot`1t between andbeengaged 'by the lips of said dies; Y

2, HighY temperature 4high pressure apparatustcomprising az pair of opposed, recessed?` pistons,vmeans for' exerting pressure against at least one of said pistons, av

pair of members, one vof said.members.'being/positioned partiallyi'within keachof said-recesses,alayer ofl insulation Ibetween one of' said members andl its` associatedpiston, an electricalconnectiontog eachoffV said members, each memberv comprising-a die, the outerface ofsaid diehaving'a raised -annular lip vdelining arecessga cylinA drical reaction vessel lo'catedfwithinthe recesses of-opposingdie faces, said reaction vessel comprising` a -hollowA conductivity cylinder adapted to contain aspecimen to lbe subjected tto high temperature high-pressure conditions in electricalfcontact with said' dies, and anlannulal gasket assembly comprisinga pluralityv of annularinsu,a lating andpressure vresisting washersi an annular metalf lic washer positioned between adjacent insulating-and pressure`V resistingy washers, said gasket assembly surrounding ,fthe side of said vesselv and havin-gf'its z outerl Aedge positioned adjacent said annular lip, the outer edgey of said gasket assembly beingarranged-to tybetwcen and be engaged7 by-the'lips` of said dies;

3. High temperature high pressure1 apparatus comprising apairv of opposed, recessed pistons, meansfop exerting pressurey against atleast oneof saidV pistons, a pair of membersone ofv said members being' positionedpartially within each of said recesses; a layerof insulation-between one of said members and its associatedfpiston3-. an-elcctrical connection to each of said members, each memberl comprising a die, at least onebinding ring-aroundY said-die, theouter faceof said die having a raised annularlip defining a recess, a block of electrically. insulating material positioned in the central portion of said recess, a reactionV vessel loca-ted within-the recesses 'of opposing k:die facesrbetween said =blocks,,saidjreacti on vessel comprising a hollow conductive cylinder adapted to contain a specimen to be subjected toY high temperature high pressure conditions in electrical contact with said dies, and an annular gasket assembly comprising a plurality of annular insulating and pressure resisting washers, an annular metallic washers, positioned between adjacent insulating and pressure resisting washers, said gasket assembly'A surrounding the sidelv ofjsaid vessel and having its outer edge positionedl adjacent said annular lip, :the outer edge of s aid gasket assembly being arranged to fit between andlbe engagedv by the lipsofj said dies.

4. High temperature high pressure apparatus compris ing a pair of opposed, recessed pistons, means for exerting pressurel against at leastV onel of said pistons, a pair of members,` one'of' said members being positioned partially within each of said recesses, a layer of insulation between one of said members and its associated piston. an. electrical; connection to@I each' of said members, :each: membencomprising-@dictanleastrone binding;- ring-s around; saidf. die.` the outer face; ofzsaidi diez having ai raised annulau liprdening a; recess; af b loclfof:`

electrically? insulating: material positioned; intv the central portion o fsaid process,- a; cylindrical reaction: vessel; located within the. recesses," o f opposing; die.; facesi between; said; blocks; said;reactionvesselfcomplrising a pair:- offsnaced; conductive; discs;v afhellow conductive? cvl adantedto contain:4 specimen-.fte befsubiected.; tog. high;` temperature highfvepressure Cenditons positioned; between.i said-k discs anzinsulating *washer* around said, cylinderfbetween said discs,Y anda-n annular gasket assembly; comprising a plurality of; annular; insulating,l and `pressureresisting.-v wash-vr ers an annular metallic washer; positionedbetween ad-v jacent: pressure. resisting washers; said: gasketv assembly surroundinglthefside oft, said: vesseL and havingritsonter edge/Positioned adiacentsaid yannular lip, thefouter edge;A

of saidgasket assembly.Y bengsarrangedto lit'betweentand. beengaged by the; lips' of., said dies;

5. A highpressurehighf temperature apparatus corn-A prising. .in c ombination,- a; pairof'opposeddies; means.l to Y move one. ofY saiiill dies.toward the:I other, each: ofv thefopfk posedlsurfacesroffsaid; dies haw/.iriglaV raised. annular. taperedlip spaced within` the-periphery ot said surfacensaidlips.

dening--arecess `to containtanobject to besubjected. to

high` pressures and high ,ternperaturegan annular thermal and'electrically insulating gasketadjacent each dieandf surro.unding .and engagingsaid object,anannularmetallic gasket between 'andincontact withsaid thermalU and elec- `trically linsulating gaskets and'surrounding said object,A

the said, insulating.'gaskets.b,eing engagedfby the lips of said dieter,` deformation thereof uponfm'ovement of`Y one of said' diesv toward the v other; andmeans `to conduct electrical current through said object for heating-thereof.

6, A`l high pressure high temperature. apparatus cornprising in cojrnbination,,ttjpalii` ofjopposeddies, means to` move one of'said dies toward'the other, eaclij'f the op; posed surfaceshofsaid vdies hayingagraised'annular tapered lip spacedwithin the'V periphery off'saidisurffac; said, lips dehing a recesstol containa'nobject to be subjected to highpressurfeslandlhigh temperatures; a block'offtherrnal and electricallyY insulatingimaterial" in'said "recess otfeachY die, and a reaction vesselpin saidrecess between' said blocks, said reaction vesselcornprisingfa hollow; thermal and electrically. insulatngcylinderjt'o,contain a specimen material therein, anV electrically conductive disc closing each end o f said hollow cylinderl and in contactwith each die,'an annular thermal and electricallyinsulating gaskety adjacent each die and surrounding andi engaging saidV reaction vessel, an, annular, metallic gasket between and engaging said thermal 1 and,v electrically insulating gaskets and surrounding said reaction vessel, the said gaskets being,-

engaged, by the lips of said ,dies yfor deformation thereof upon ,movement` o fone otsaid'dies toward the other, and means o tol v conductall- ,electrical curr/,entI through said re. action vessel; s

(References on following page) References Cited in the le of this patent UNITED STATES PATENTS Bridgman et a1. Mar. 6, 19511 OTHER REFERENCES 5 Parsons: Philosophical Transactions of the Royal Society, v01. 220, Series A (1919), pages 67-75, 85-87, 92-101.

Bridgman: Am. Acad. of Arts and Sciences, Prceedings, vol. 74, No. 3, pages 21-28, October 1940.

Gunther et al.: Z. anorg. allgem. chem, vol. 256, pages 357-372 (1943).

Bridgman: Reviews of Modern Physics, vol. 18, No. 1, pages 1-9, 25, 34, 79-88 (1946).

Bridgman: J Chem. Physics, vol. 15, No.2 (February 1947), Pages 92-98. 

